CN107626915B - A kind of the micro-nano aluminium powder/porous carbon composite material and its synthetic method of acid and alkali-resistance - Google Patents
A kind of the micro-nano aluminium powder/porous carbon composite material and its synthetic method of acid and alkali-resistance Download PDFInfo
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Abstract
The invention discloses a kind of micro-nano of acid and alkali-resistance aluminium powder/porous carbon composite material and its synthetic methods, this method is mainly characterized by devising a kind of composite solvent system dissolution carbon precursor first and disperses aluminium powder raw material, the composite solvent system parts by weight are 30~50, and following weight parts constitutive material: micro-nano aluminium powder 30~40 is then added；Charcoal source 20~30.The invention also discloses the preparation methods of the material, and the material organic matter volatile contents are few, are conducive to environmental protection, have good resistance to acid and alkali, wearability, and long service life, storage stability is good, easy to operate, are suitble to large-scale industrial production.
Description
Technical field
The present invention relates to composite materials, the field of the aluminium powder containing energy, and in particular to a kind of micro-nano aluminium powder/porous charcoal of acid and alkali-resistance is multiple
Condensation material and its synthetic method.
Background technique
Common aluminium powder product is widely used in chemical catalyst, pesticide, anti-corrosion material, metallized coating, conductive coating, adds
Gas concrete foaming agent, deoxidizer in steel production, refractory material, aluminothermic process alloy, thermal spraying composite powder etc..And nanoscale aluminium
Material has special optical characteristics, electrology characteristic and chemical reactivity, in new rocket propellant, explosive wastewater and solar battery
Etc. high-tech areas applied.
Nanometer aluminium powder has special surface and interface effect, and surface atom is more, and surface atom can be with nano aluminum
The reduction of powder diameter and increase；And the specific surface area and specific surface energy of nanometer aluminium powder are all very big.Above-mentioned two factor is all led
Cause nanometer aluminium powder reactivity very high, especially when exposed to air its surface atom very sensitive to locating environment
Easily it is oxidized to form fine and close and hard Al2O3, the oxide shell layer of formation are coated on the surface of nanometer aluminium powder, this will be serious
The activity of nanometer aluminium powder is influenced, and the oxide generated does not contribute combustion reaction, can reduce nanometer aluminium powder instead
Incendiary effect.So how to keep the activity of nanometer aluminium powder, the generation of oxide is prevented, nanometer aluminium powder can be controlled well
Active release becomes the research hotspot in the field.
Holding active for nanometer aluminium powder is largely that in-situ treatment is carried out from the surface of nano-aluminium particle, most important
The processing of nanometer aluminium powder surface cladding is carried out, to make internal disorder or usurp be most widely oxide cladding, polymer overmold, metal simple-substance packet wherein grinding
It covers, propellant component cladding and charcoal bag are covered.Wherein charcoal cladding coats one layer of charcoal shell on the surface of nano-aluminium particle with shape
At the core-shell structure of charcoal cladding aluminium, most directly effect is to completely cut off connecing for kernel aluminium and outside air to the charcoal shell on nanometer aluminium powder surface
Touch the activity to keep nanometer aluminium powder；In addition, layer of charcoal can burn rapidly under the conditions of high fever, kernel aluminium is exposed to high fever ring
It burns in border, the burning of layer of charcoal provides additional energy, improves the enthalpy of combustion of nanometer aluminium powder indirectly.Charcoal cladding for
It is a kind of ideal surface cladding for nanometer aluminium powder, charcoal shell property in low temperature is stablized, can be with effective protection nanometer aluminium powder
Activity；In high-temp combustion, charcoal shell, which participates in reaction, can provide additional combustion enthalpy.
Using ethyl orthosilicate as presoma, ammonium hydroxide is catalyst, is wrapped using sol-gel method on thin slice aluminium powder pigment surface
One layer of thin and compact nanosized SiO_2 layer has been covered, has been the most common method for coating, the SiO2 of this method preparation coats aluminium powder material
With good acid resistance, but alkali resistance is very poor.SiO2 cladding process resistance to corrosion is strong, but SiO2 is likely to from solution
It is precipitated out to form nano particle, and heterogeneous flocculation occurs with Al powder (stratum nucleare) particle, form irregular cladding
Carbon coating Al nanoparticle is prepared under the atmosphere of CH4 gas and Ar gas using laser-induction composite heating method, it is former
Reason is: METAL HEATING PROCESS being melted to high-frequency induction and reached higher temperature, significantly improves metal to the absorptivity of laser, favorably
In the effect for giving full play to laser；Being re-introduced into laser evaporates metal rapidly, and generates very big temperature and barometric gradient, but this
A little methods are there is also certain shortcoming, and there are some aluminium oxide for the charcoal cladding nanometer aluminium powder that these methods obtain, and it is miscellaneous to carbonize aluminium
Matter exists, and core-shell particles size is difficult to control, and vulnerable to ambient humidity, temperature influence and lose activity, energy consumption is high, explosive
Fried, complex process, the technological deficiencies such as equipment is expensive, production scale is small, product form is uncontrollable.
Summary of the invention
The purpose of the present invention is to provide a kind of micro-nano of acid and alkali-resistance aluminium powder/porous carbon composite material and its synthetic methods；
Micro-nano aluminium powder prepared by the present invention/porous carbon composite material acid-fast alkali-proof performance is good, substantially increases the heat of aluminium powder
Value, and have no effect on the activity of aluminium powder.
The present invention is achieved by the following technical solutions:
Micro-nano aluminium powder/porous carbon composite material of acid and alkali-resistance, including composite solvent system 30~50, micro-nano aluminium powder 30~
40, charcoal source 20~30；The composite solvent system is made of the raw material of following weight parts:
Main solvent 20~30；
Secondary solvent 5~10；
Wetting dispersing agent 3~6；
Levelling agent 1.5~2.5；
Coupling agent 0.3~0.8；
Anti-settling agent 0.2~0.7；
The main solvent be ethyl acetate, n-butyl acetate, isobutyl acetate, pentyl acetate, ethyl lactate, acetone,
Butanone, propione, isobutyl methyl ketone, cyclohexanone, ethyl alcohol, isopropanol, isobutanol, one or more of cyclohexanol group
It closes.
The secondary solvent is the combination of one or more of propylene glycol methyl ether acetate, turkey red oil, palm oil.
The wetting dispersing agent is lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, polyacrylamide, gathers
The combination of one or more of ethylene glycol.
The levelling agent be 201 methyl-silicone oils, 205 active methyl silicone oil, BYK-300, BYK-301, BYK-320,
The combination of one or more of BYK-VP-330.
The coupling agent be KH-550, KH-560, KH-570, KH-151, KH-171, TTOP-12 titanate coupling agent,
One or more of TC-1, TC-3, YB-401 combination.
The anti-settling agent is polyglycerol polyricinoleate, polyethylene wax, organobentonite, gas phase SiO2One of or two
Kind or more combination.
The carbon precursor is phenolic resin, epoxy resin, alkyd resin, polyester resin, acrylic resin, grape
The combination of one or more of sugar, fructose, maltose, sucrose, chitosan.
Micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance, comprising the following steps:
(1) ingredient: according to formula metering each component；
(2) composite solvent system is designed first, and main solvent and secondary solvent are put into stirred tank and are sufficiently stirred, is opened
Begin 2000~3000r/min of speed regulation, and temperature is controlled at 50~60 DEG C, after being uniformly dispersed, by mixing speed compared with as low as 500~
1000 r/min are successively added dropwise to dispersing agent and coupling agent under agitation, anti-settling agent are added after to be cooled to 30~40 DEG C
And levelling agent, it stirs 20~30 minutes；
(3) micro-nano aluminium powder and charcoal source are then each sequentially added to above-mentioned dicyandiamide solution, divided in supersonic generator
Processing 45~60 minutes is dissipated, is dried 1~2 hour under the conditions of 80~100 DEG C and obtains aluminium base presoma；
(4) finally by obtained aluminium base presoma, high temperature carbonization is handled under inert gas protection, obtains micro-nano aluminium powder/more
Hole carbon composite.
Inert gas used in the step (4) is the mixed gas such as nitrogen-hydrogen or argon gas-hydrogen, is led to
The angle of incidence terminates from beginning to warm up to reaction.
The temperature of step (4) the high temperature charing is 600~1000 DEG C, and the time is 2 hours, wherein the 1st hour
Interior heating rate is 10~15 DEG C of min–1；Heating rate in 2nd hour is 15~20 DEG C of min–1。
Beneficial effects of the present invention:
1, nano-powder generates in high-purity inert gas, thus purity is very high, and resistance to acid and alkali is good, organic solvent volatilization
It is few, be conducive to green production.
2, the metallic vapour substrate surface smooth on surface is initially formed nano thin-film in homogeneous thickness, then obtains through shedding is broken
Nano-powder, thus epigranular, surfacing rule, well-crystallized；
3, granularity is easily controllable, the type, pressure and the flow velocity that change inert gas and cooling temperature can be borrowed real
It is existing.
Detailed description of the invention
Fig. 1 is micro-nano aluminium powder and micro-nano aluminium powder/porous carbon composite X-ray diffractogram, and 1 is micro-nano aluminium powder in figure, and 2 are
Micro-nano aluminium powder/porous carbon composite.
Fig. 2 is liberation of hydrogen curve in acid condition.
Fig. 3 is liberation of hydrogen curve under alkaline condition.
Specific implementation method
Embodiment 1:
A kind of micro-nano aluminium powder/porous carbon composite material of acid and alkali-resistance, is prepared by the component raw material of following weight (kg):
Aluminium powder 30, phenolic resin 25, ethyl acetate 25, propylene glycol methyl ether acetate 12, carboxymethyl cellulose 6；
BYK-300 1.5；KH-550 0.3；Polyethylene wax 0.2；
Preparation method includes the following steps:
(1) composite solvent system is designed first, and ethyl acetate and propylene glycol methyl ether acetate are put into stirred tank
It is sufficiently stirred, starts to adjust the speed 2000r/min, temperature is controlled at 50 DEG C, after being uniformly dispersed, by mixing speed compared with as low as 500r/
Min, is successively added dropwise to carboxymethyl cellulose and KH-550 under agitation, be added after to be cooled to 30 DEG C polyethylene wax and
BYK-300 is stirred 20 minutes；
(2) then aluminium powder and phenolic resin are each sequentially added to above-mentioned dicyandiamide solution, ultrasonic disperse is handled 45 minutes.
It is dried 1 hour under the conditions of 80 DEG C and obtains aluminium base presoma；
(3) finally by obtained aluminium base presoma, 800 DEG C of high temperature carbonizations are handled 2 hours under nitrogen-hydrogen protection, are obtained
Micro-nano aluminium powder/porous carbon composite material.
Embodiment 2:
A kind of aluminium powder/porous carbon composite material of acid and alkali-resistance, is prepared by the component raw material of following weight (kg):
Aluminium powder 35, epoxy resin 27, acetone 20, palm oil 10, polyacrylamide 5；BYK-331 2 ；KH-560
0.5；Organobentonite 0.5；
Preparation method includes the following steps:
(1) composite solvent system is designed first, and acetone and palm oil are put into stirred tank and are sufficiently stirred, starts to adjust
Fast 2500r/min, temperature is controlled at 55 DEG C, after being uniformly dispersed, by mixing speed compared with as low as 800 r/min, in stirring condition
Under be successively added dropwise to polyacrylamide and KH-560, organobentonite and BYK-331 are added after to be cooled to 35 DEG C, stirs 25 points
Clock；
(2) then aluminium powder and epoxy resin are each sequentially added to above-mentioned dicyandiamide solution, ultrasonic disperse is handled 50 minutes,
It is dried 1.5 hours under the conditions of 90 DEG C and obtains aluminium base presoma；
(3) finally by obtained aluminium base presoma, 900 DEG C of high temperature carbonizations are handled 2 hours under nitrogen-hydrogen protection, are obtained
Micro-nano aluminium powder/porous carbon composite material.
Embodiment 3:
A kind of micro-nano aluminium powder/porous carbon composite material of acid and alkali-resistance, is prepared by the component raw material of following weight (kg):
Aluminium powder 40, glucose 20, ethyl alcohol 25, turkey red oil 8, polyethylene glycol 4；201 methyl-silicone oils 2；YB-401 0.7；Gather sweet
Oily polyricinoleate 0.3；
(1) composite solvent system is designed first, and ethyl alcohol and turkey red oil are put into stirred tank and are sufficiently stirred, starts to adjust
Fast 3000r/min, temperature is controlled at 60 DEG C, after being uniformly dispersed, by mixing speed compared with as low as 1000 r/min, in stirring condition
Under be successively added dropwise to polyethylene glycol and YB-401, polyglycerol polyricinoleate and methyl-silicone oil, stirring are added after to be cooled to 40 DEG C
30 minutes；
(2) then aluminium powder and glucose are each sequentially added to above-mentioned composite solvent system, ultrasonic disperse handles 60 points
Clock.It is dried 2 hours under the conditions of 100 DEG C and obtains aluminium base presoma；
(3) finally by obtained aluminium base presoma, 1000 DEG C of high temperature carbonizations are handled 2 hours under argon gas-hydrogen shield, are obtained
To micro-nano aluminium powder/porous carbon composite material.
Embodiment 4:
A kind of aluminium powder/porous carbon composite material of acid and alkali-resistance, is prepared by the component raw material of following weight (kg):
Aluminium powder 35, acrylic resin 26, isobutanol 20, propylene glycol methyl ether acetate 10, polyethylene glycol 6；BYK-VP-330
2；TC-1 0.4；Polyethylene wax 0.6；
Preparation method includes the following steps:
(1) composite solvent system is designed first, and isobutanol and propylene glycol methyl ether acetate are put into stirred tank and filled
Divide stirring, starts to adjust the speed 3000r/min, temperature is controlled at 60 DEG C, after being uniformly dispersed, by mixing speed compared with as low as 1000 r/
Min is successively added dropwise to polyethylene glycol and TC-1 under agitation, polyethylene wax and BYK-VP- is added after to be cooled to 40 DEG C
330, it stirs 30 minutes；
(2) then aluminium powder and acrylic resin are each sequentially added to above-mentioned composite solvent system, ultrasonic disperse processing
It 60 minutes, is dried 1.5 hours under the conditions of 80 DEG C and obtains aluminium base presoma；
(3) finally by obtained aluminium base presoma, 900 DEG C of high temperature carbonizations are handled 2 hours under argon gas-hydrogen shield, are obtained
Micro-nano aluminium powder/porous carbon composite material.
Embodiment 5:
A kind of micro-nano aluminium powder/porous carbon composite material of acid and alkali-resistance, is prepared by the component raw material of following weight (kg):
Aluminium powder 30, maltose 24, cyclohexanone 26, propylene glycol methyl ether acetate 12, lauryl sodium sulfate 6；BYK-
320 1.5；KH-171 0.3；Gas phase SiO20.2；
Preparation method includes the following steps:
(1) composite solvent system is designed first, and cyclohexanone and propylene glycol methyl ether acetate are put into stirred tank and filled
Divide stirring, starts to adjust the speed 2000r/min, temperature is controlled at 60 DEG C, after being uniformly dispersed, by mixing speed compared with as low as 600r/
Min is successively added dropwise to lauryl sodium sulfate and KH-171 under agitation, gas phase SiO is added after to be cooled to 30 DEG C2With
BYK-320 is stirred 20 minutes；
(2) then aluminium powder and maltose are each sequentially added to above-mentioned dicyandiamide solution, ultrasonic disperse is handled 40 minutes,
It is dried 1 hour under the conditions of 70 DEG C and obtains aluminium base presoma；
(3) finally by obtained aluminium base presoma, 800 DEG C of high temperature carbonizations are handled 2 hours under nitrogen-hydrogen protection, are obtained
Micro-nano aluminium powder/porous carbon composite material.
Embodiment 6:
A kind of micro-nano aluminium powder/porous carbon composite material of acid and alkali-resistance, is prepared by the component raw material of following weight (kg):
Aluminium powder 30, chitosan 25, butanone 25, turkey red oil 12, methyl anyl alcohol 5；BYK-301 2；TTOP-12 0.4；
Polyethylene wax 0.6；
Preparation method includes the following steps:
(1) composite solvent system is designed first, and butanone and turkey red oil are put into stirred tank and are sufficiently stirred, starts to adjust
Fast 2500r/min, temperature is controlled at 60 DEG C, after being uniformly dispersed, by mixing speed compared with as low as 600r/min, under agitation
It is successively added dropwise to methyl anyl alcohol and TTOP-12, polyethylene wax and BYK-301 is added after to be cooled to 40 DEG C, stirs 30 minutes；
(2) then aluminium powder and chitosan are each sequentially added to above-mentioned dicyandiamide solution, ultrasonic disperse is handled 45 minutes.?
It is dried 1 hour under the conditions of 60 DEG C and obtains aluminium base presoma；
(3) finally by obtained aluminium base presoma, 700 DEG C of high temperature carbonizations are handled 2 hours under nitrogen-hydrogen protection, are obtained
Micro-nano aluminium powder/porous carbon composite material.
Claims (10)
1. a kind of micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance, which is characterized in that the acid and alkali-resistance it is micro-
Aluminium powder/porous carbon composite material of receiving includes the raw material of following parts by weight: composite solvent system 30~50, micro-nano aluminium powder 30~40,
Charcoal source 20~30；
The composite solvent system is made of the raw material of following weight parts:
Main solvent 20~30；
Secondary solvent 5~10；
Wetting dispersing agent 3~6；
Levelling agent 1.5~2.5；
Coupling agent 0.3~0.8；
Anti-settling agent 0.2~0.7；
Micro-nano aluminium powder/porous carbon composite material synthetic method of the acid and alkali-resistance, comprising the following steps:
(1) ingredient: according to formula metering each component；
(2) composite solvent system is designed first, and main solvent and secondary solvent are put into stirred tank and are sufficiently stirred, starts to adjust
2000~3000r/min of speed, temperature are controlled at 50~60 DEG C, and after being uniformly dispersed, mixing speed is reduced to 500~1000
R/min, is successively added dropwise to wetting dispersing agent and coupling agent under agitation, be added after to be cooled to 30~40 DEG C anti-settling agent and
Levelling agent stirs 20~30 minutes；
(3) micro-nano aluminium powder and charcoal source are then each sequentially added to above-mentioned composite solvent system, ultrasonic disperse processing 45~60
Minute, it is dried 1~2 hour under the conditions of 80~100 DEG C and obtains aluminium base presoma；
(4) finally by obtained aluminium base presoma, high temperature carbonization is handled under inert gas protection, obtains micro-nano aluminium powder/porous charcoal
Composite material.
2. micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance according to claim 1, feature exist
In, the main solvent be ethyl acetate, n-butyl acetate, isobutyl acetate, pentyl acetate, ethyl lactate, acetone, butanone,
Propione, isobutyl methyl ketone, cyclohexanone, ethyl alcohol, isopropanol, isobutanol, the combination of one or more of cyclohexanol.
3. micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance according to claim 1, feature exist
In the secondary solvent is the combination of one or more of propylene glycol methyl ether acetate, turkey red oil, palm oil.
4. micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance according to claim 1, feature exist
In the wetting dispersing agent is lauryl sodium sulfate, methyl anyl alcohol, cellulose derivative, polyacrylamide, polyethylene glycol
One or more of combination.
5. micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance according to claim 1, feature exist
In the levelling agent is 201 methyl-silicone oils, 205 active methyl silicone oil, BYK-300, BYK-301, BYK-320, BYK-VP-
One or more of 330 combination.
6. micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance according to claim 1, feature exist
In, the coupling agent be KH-550, KH-560, KH-570, KH-151, KH-171, TTOP-12 titanate coupling agent, TC-1,
One or more of TC-3, YB-401 combination.
7. micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance according to claim 1, feature exist
In the anti-settling agent is polyglycerol polyricinoleate, polyethylene wax, organobentonite, gas phase SiO2One or both of with
On combination.
8. micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance according to claim 1, feature exist
In the charcoal source is phenolic resin, epoxy resin, alkyd resin, polyester resin, acrylic resin, glucose, fructose, wheat
The combination of one or more of bud sugar, sucrose, chitosan.
9. micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance according to claim 1, feature exist
In inert gas used in the step (4) is nitrogen-hydrogen or argon gas-hydrogen mixed gas, is passed through the time
Terminate from beginning to warm up to reaction.
10. micro-nano aluminium powder/porous carbon composite material synthetic method of acid and alkali-resistance according to claim 1, feature exist
In the temperature of the step (4) high temperature charing is 600~1000 DEG C, and the time is 2 hours, wherein the liter in the 1st hour
Warm rate is 10~15 DEG C of min–1；Heating rate in 2nd hour is 15~20 DEG C of min–1。
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